HPLC法测定盐酸表阿霉素-索拉非尼PLGA栓塞微球的载药量和包封产率  

Determination of Drug Loading and Encapsulation Efficiency of Epirubicin Hydrochloride-sorafenib PLGA Embolic Microspheres by HPLC

作　　者：刘斌斌[1] 简晖[1,2] 黄珊珊[1] 刘微[2] 朱益雷 罗晓健[1,2] 李翔[1,2] LIU Binbin JIAN Hui HUANG Shanshan LIU Wei ZHU Vilei LUO Xiaojian LI Xiang(College of Pharmacy, Jiangxi University of TCM, Nanchang 330006, China National Pharmaceutical Engineering Center for TCM Solid Preparation, Nanchang 330006, China)

机构地区：[1]江西中医药大学药学院,南昌330006 [2]中药固体制剂制造技术国家工程研究中心,南昌330006

出　　处：《中国药房》2017年第21期2967-2970,共4页China Pharmacy

基　　金：国家自然科学基金资助项目(No.81603054);江西省卫生计生委中医药科研课题(No.2016A008);江西省博士后科研项目(No.2016KY08)

摘　　要：目的:建立测定盐酸表阿霉素-索拉非尼聚乳酸-羟基乙酸聚合物(PLGA)栓塞微球载药量和包封产率的方法。方法:采用高效液相色谱法测定该制剂中盐酸表阿霉素和索拉非尼的含量,再通过公式计算载药量和包封产率。色谱柱为Phenomenex Luna 5u C8(2)100A,流动相为甲醇-[水(含0.05%三氟乙酸和0.14%十二烷基硫酸钠)](75∶25,V/V),流速为1.0 mL/min,检测波长为252 nm,柱温为25℃,进样量为10μL。结果:盐酸表阿霉素和索拉非尼检测质量浓度线性范围分别为2.020~101.00μg/mL(r=0.999 8)、2.048~102.40μg/mL(r=0.999 7);定量限分别为3.297 0、2.546 8μg/mL;检测限分别为0.989 1、0.764 1μg/mL;精密度、稳定性、重复性试验的RSD<2.0%;回收率分别为96.41%~101.80%(RSD=1.64%,n=9)、99.46%~101.45%(RSD=0.70%,n=9)。3批样品中两种成分的载药量≥1.17%,包封产率≥58%。结论:该方法操作简单、结果准确,可用于测定盐酸表阿霉素-索拉非尼PLGA栓塞微球的载药量和包封产率。OBJECTIVE： To establish a method for the determination of drug loading and encapsulation efficiency of Epirubicin hydrochloride-sorafenib-loaded Polylactic Acid-glycolic Acid Polymer （PLGA） embolic microspheres. METHODS： HPLC method was adopted to determine the contents of epirubicin hydrochloride and sorafenib in the preparation, and then drug loading and encapsulation efficiency were calculated by formula. The determination was performed on Phenomenex Luna 5u C8（2） 100A column with mobile phase consisted of methanol-water （containing 0.05% trifluoroacetic acid and 0.14% dium dodecyl sulfate） （75 ∶ 25,V/V） at the flow rate of 1.0 mL/min. The detection wavelength was set at 252 nm, and the column temperature was maintained at 25 ℃. The injection volume was 10 μL. RESULTS： The linear ranges were 2.020-101.00 μg/mL for epirubicin hydrochloride （r=0.999 8） and 2.048-102.40 μg/mL for sorafenib （r=0.999 7）, respectively. The limits of quantification were 3.297 0, 2.546 8 μg/mL, respectively. The detection limits were 0.989 1, 0.764 1 μg/mL, respectively. RSDs of precision, stability and repeatability tests were all less than 2.0%. The recoveries were 96.41%-101.80%（RSD=1.64%,n=9）, 99.46%-101.45%（RSD=0.70%,n=9）, respectively. Drug loading of two components in 3 batches of samples were no lower than 1.17%,encapsulation efficiency no lower than 58%. CONCLUSIONS： The method is simple, accurate, can be used to determine drug loading and encapsulation efficiency of Epirubicin hydrochloride-sorafenib PLGA embolic microspheres.

关 键 词：盐酸表阿霉素 索拉非尼 聚乳酸-羟基乙酸聚合物 栓塞微球 高效液相色谱法 载药量 包封产率 

分 类 号：R917[医药卫生—药物分析学]